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“Invent a New India Using Knowledge”

है”ह”ह

IS 14433-1 (1997): Infant milk substitutes, Part 1: MilkProtein Based [FAD 19: Dairy Products and Equipment]

IS 14433 (Part 1) : 1997Edition 1.2

(1998-12)

B U R E A U O F I N D I A N S T A N D A R D SMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

Price Group 6

© BIS 2003

Indian Standard

INFANT MILK SUBSTITUTES — SPECIFICATIONPART 1 MILK PROTEIN BASED

(Incorporating Amendment Nos. 1 & 2)

ICS 67.100.99

Dairy Products and Equipment Sectional Committee, FAD 57

FOREWORD

Human milk ideally fulfils the need for growth and additionally provides unique bio-immune factorsfor protecting the health of infants. Breast feeding is, therefore, universally regarded as the mostappropriate form of nourishing the infant. However, when breast feeding is not possible, reliance hasto be placed upon the alternate sources of nutrients for infant feeding. It is imperative that infantmilk substitutes should be properly formulated so that nutritional requirements for optimal growthare met adequately, and that there is minimum of physiological stress on the developing organs andenzymic system of the infant. It is equally important to promote correct feeding practices, so thatappropriate use of the infant milk substitute could be made for protecting the health of the infant.Under the Infant Milk Substitutes, Feeding Bottles and Infant Foods ( Regulation of Production,Supply and Distribution ) Act, 1992, various types of foods for infants being marketed in ourcountry have been placed under the following two categories:

a) Infant Milk Substitutes, andb) Infant Foods.

‘Infant Milk Substitute’ means any food being marketed or otherwise represented as partial ortotal replacement for mother’s milk, whereas ‘Infant Food’ means any food being marketed orotherwise represented as a complement to mother’s milk to meet the growing nutritional needs ofthe infant after the age of four months.Earlier, the requirements of infant milk substitutes were covered under separate standards,namely, IS 1547 ‘Infant milk food’ and IS 11156 ‘Infant formulae’. While reviewing thesestandards for alignment with the Infant Milk Substitutes, Feeding Bottles and Infant Foods( Regulation of Production, Supply and Distribution ) Act, 1992, it was decided to revise thesestandards, amalgamating them into one comprehensive standard. Part 1 of this standard coversInfant Milk Food and Infant Formulae which are primarily milk protein based, whereas Part 2 ofthis standard is intended to cover vegetable protein based infant milk substitutes. Consequently,Part 1 of this standard would supersede IS 1547 : 1985 and IS 11156 : 1985.The present amalgamated revision is also being carried out in view of the following:

a) For harmonization of the standard with statutory rules and regulations.b) For safeguarding the health of the infants, the bacteriological requirements have been made

more stringent.c) For incorporating the amendments issued so far, with changes as required in accordance with

the statutory rules and regulations.While formulating this standard, due consideration has been given to the relevant rules prescribedby the Government of India, namely Rule 37-A, 37-B, 49( 19 ) and items under Appendix B ofPrevention of Food Adulteration Rules 1955; Infant Milk Substitutes, Feeding Bottles and InfantFoods ( Regulation of Production, Supply and Distribution ) Act, 1992 and Rules 1993; Rule 5 and‘Third Schedule’ of the Standards of Weights and Measures ( Packaged Commodities ) Rules, 1977.

NOTE — The various Statutory rules indicated were valid at the time of publication of this standard. Since theStatutory rules and Acts are updated from time to time, this standard is subject to the restrictions imposed under theseActs and Rules wherever applicable.

A scheme for labelling environment friendly products known as ECO-Mark has been introduced atthe instance of the Ministry of Environment and Forests (MEF), Government of India. TheECO-Mark shall be administered by the Bureau of Indian Standards (BIS) under the BIS Act,1986 as per the Resolution No. 71 dated 20 February 1991 and No. 425 dated 28 October 1992published in the Gazette of the Government of India. For a product to be eligible for marking withthe ECO Mark, it shall also carry the Standard Mark of BIS for quality besides meeting additionalenvironment friendly (EF) requirements given in the standard, which are based on the GazetteNotification No. GSR 624 (E) dated 6 September 1995 for Labelling Beverages. Infant Foods andProcessed Fruits and Vegetable Products as Environment Friendly Products, published in theGazette of the Government of India.This edition 1.2 incorporates Amendment No. 1 (November 1997) and Amendment No. 2(December 1998). Side bar indicates modification of the text as the result of incorporation of theamendments.For the purpose of deciding whether a particular requirement of this standard is complied with,the final value, observed or calculated, expressing the result of a test or analysis, shall be roundedoff in accordance with IS 2 : 1960 ‘Rules for rounding off numerical values ( revised )’. The numberof significant places retained in the rounded off value should be the same as that of the specifiedvalue in this standard.

IS 14433 (Part 1) : 1997

1

Indian Standard

INFANT MILK SUBSTITUTES — SPECIFICATIONPART 1 MILK PROTEIN BASED

1 SCOPE

This standard (Part 1) prescribes the types,requirements, methods of test and sampling formilk protein based, infant milk substitutes.

2 REFERENCES

The Indian Standards listed in Annex Acontain provisions which through reference inthis text, constitute provision of this standard.At the time of publication, the editionsindicated were valid. All standards are subjectto revision and parties to agreements based onthis standard are encouraged to investigate thepossibility of applying the most recent editionsof the standards indicated.

3 TERMINOLOGY

For the purpose of this standard, the followingdefinitions shall apply.3.1 Infant Milk Food

The material as prepared by spray drying or byroller drying of the milk of cow or buffalo or amixture thereof. The milk may be modified bythe partial removal/substitution of differentmilk solids, carbohydrates such as sucrose,dextrose and dextrins, maltose and lactose,salts such as phosphates, citrates; vitamins A,D, E, B group C, and other vitamins, mineralssuch as iron, copper, zinc, iodine and others.3.2 Infant Formula

The material as prepared by spray drying orroller drying of the milk of cow or buffalo or amixture thereof. The milk may be modified bythe partial removal/substitution of milk fatwith edible vegetable oils rich inpolyunsaturated fatty acids and/or by differentmilk solids, either singly or in a suitablecombination; carbohydrates such as sucrose,dextrose and dextrins, maltose and lactose;salts such as phosphates, citrates; vitamins A,D, E, B group C, and other vitamins; mineralssuch as iron, copper, zinc, iodine and others.

NOTE — Infant Formula meant for infants with lowbirth weight (less than 2 500 g) and suitably modifiedwith addition of proteins, whey proteins, minerals so asto achieve the required whey : casein ratio; calcium :phosphorus ratio along with other requirements, asgiven in the standard, shall be termed as Low BirthWeight Infant Milk Substitute.

3.3 Infant

A child not more than 12 months of age.

3.4 Routine Tests

Tests carried out on each lot to check theessential requirements which are likely to varyduring production.3.5 Type Test

The tests to prove conformity to therequirements of this standard. They areintended to approve the formulation andquality of the product at least in the beginningof marketing or certification or both. Thesetests are also conducted periodically tosupplement the routine tests or whenever thebasic formula or method is changed.

4 TYPES

4.1 The material shall be of the following twotypes:

5 DESCRIPTION

5.1 The product shall be white or white with agreenish tinge to light cream in colour,reasonably free from lumps and shall beuniform in appearance.

6 REQUIREMENTS

6.1 Type 1 Infant Milk Substitute shall be freefrom starch and added antioxidants while inType II, ready to drink infant milk substitute,lecithin ( see IS 5055 : 1996 ) and ascorbylpalmitate ( see IS 13462 : 1992 ) may be usedup to a maximum limit of 0.5 g/100 ml and1 mg/100 ml respectively and shall be free fromstarch. It shall also be free from dirt, andextraneous matter, preservatives, added colourand flavour and from any material which areharmful to infant’s health.6.2 The flavour of the product in dry conditionor of the reconstituted feed shall be fresh andsweet. The material shall not have any rancidtaste or musty odour ( see IS 10641 : 1983 ).6.3 The scorched particles in the product shallnot exceed 15 mg (equivalent to Disc B) whentested as per the method given inIS 13500 : 1992.

a) Type I —Infant milk food, andb) Type II —Infant formula including Low

Birth Weight Infant MilkSubstitute:

i) Infant formulaii) Low Birth Weight Infant Milk

Substitute.

IS 14433 (Part 1) : 1997

2

6.4 For Type II Infant milk substitutes,vegetable oils added shall be rich inpolyunsaturated fatty acids. It shall alsocontain a minimum linoleate (linoleic acid inform of glycerides) content of 1.398 g per 100 gof the product when determined as per themethod given in Annex A of IS 6387 : 1987. Theproduct shall also contain a minimum of 0.7 IUof vitamin E per 100 kcal, when determined asper the method given in IS 7235 : 1974.6.5 Quality of Ingredients

6.5.1 All ingredients used shall be clean, ofgood quality, safe and suitable for ingestion byinfants.6.5.2 The vitamins and minerals shall be offood grade. Iron salts should be such so as toensure high bio-availability of iron. The sourceof iron may be selected from ferrous citrate;ferrous fumarate; ferrous succinate, ferroussulphate; ferric ammonium citrate and ferricpyrophosphate.6.6 Hygienic Conditions

The material shall be manufactured andpacked under hygienic conditions ( see IS 2491 :1972 ).6.7 Bacteriological Requirements

6.7.1 Bacterial CountThe bacterial colony count per gram of theproduct shall not be more than 40 000 whendetermined according to the method prescribedin IS 5402 : 1969.6.7.2 Coliform CountThe coliform bacteria shall be absent per 0.1 gof the product when determined according tothe method prescribed in IS 5401 : 1969.6.7.3 Staphylococcus aureusStaphylococcus aureus shall be absent per 0.1 gof the product when tested as per the methodprescribed in IS 5887 (Part 2) : 1976.6.7.4 Salmonella and ShigellaSalmonella and Shigella shall be absent per25 g of the product when tested as per themethod prescribed in IS 5887 (Part 3) : 1976( see Note ).

NOTE — The requirements for Salmonella and Shigellashall be tested in a laboratory situated away from theproduction area.

6.8 The Infant milk substitutes shall alsoconform to requirements given in Table 1.6.8.1 The Low Birth Weight Infant MilkSubstitute shall meet the requirementsprescribed under 6.8.1.1 to 6.8.1.3 in additionto the requirements prescribed for Type IIInfant Milk Substitute under 6 and Table 1.

6.8.1.1 Protein content shall be 2.25 g/100 kcal/Jto 2.75 g/100 kcal/J, when determined as per themethod prescribed in IS 7219 : 1973.6.8.1.2 Mineral content shall not be less than0.5 g/100 kcal. The Calcium Phosphorus ratioshall be 2 : 1 when determined as per themethods prescribed in IS 5949 : 1990 andIS 12756 : 1989 respectively. Sodium,Potassium and Chloride combined togethershall not be less than 40 milliequivalent per litrewhen determined as per the methods prescribedin IS 12760 : 1989 and IS 11763 : 1986.6.8.1.3 Whey : Casein ratio shall be 60 : 40.Essential amino acids should include Cystine,Tyrosine and Histidine.

NOTES

1 1 kJ = 0.238 846 kcal or 1 kcal = 4.186 8 kJ.

2 For the conversion of the values of requirements of thecharacteristics from percent by mass (per 100 g) to thevalue per 100 kcal, the total kcal content of the food shallbe based upon the values of 4 kcal per g of carbohydratesand per g of proteins; and 9 kcal per g of fat.Carbohydrates may be determined as per the methodprescribed under Annex C of IS 1656 : 1997.

3 The Dairy Products and Equipment SectionalCommittee, FAD 57, is in the process of identifying themethod of test for determination of whey : casein ratio.Till such time the method of test is identified, themanufacturers would be required to maintain recordsshowing compliance with the stated requirement.

6.9 Optional Requirements for ECO-Mark

6.9.1 General Requirements6.9.1.1 The product shall conform to therequirements prescribed under 6.1 to 6.8.6.9.1.2 The manufacturer shall produce theconsent clearance as per the provisions of Water( PCP ) Act, 1974, Water ( PCP ) Cess Act, 1977and Air ( PCP ) Act, 1981 alongwith theauthorization if required under Environment( Protection ) Act, 1986 and the Rules madethereunder to the Bureau of Indian Standards,while applying for the ECO-MARK and theproduct shall also be in accordance with thePrevention of Food Adulteration Act, 1954 andthe Rules made thereunder. Additionally, FPO,1955 (Fruit Product Order) framed underEssential Commodities Act, 1966, Standards ofWeights and Measures Act, 1977 and 1985requirements wherever applicable, has to becompiled with.6.9.1.3 The product/packaging may also displayin brief the criteria based on which the producthas been labelled environment friendly.6.9.1.4 The material used for product packingshall be recyclable or biodegradable.6.9.1.5 The date of manufacture and date ofexpiry shall be declared on the product packageby the manufacturer.

IS 14433 (Part 1) : 1997

3

6.9.1.6 The product shall be microbiologicallysafe when tested as per IS 5403 : 1969 andIS 5887 (Part 5) : 1976 and should be free frombacterial and fungal toxins.

6.9.1.7 The pesticide residues (if any) in theproduct shall not exceed the limit as prescribedin PFA Act, 1954 and the Rules madethereunder.

6.9.1.8 The product package or leafletaccompanying it may display instruction ofproper use, storage and transport (includingrefrigeration temperature compliance) so as tomaximize the product performance, safety andminimize wastage.

6.9.2 Specific Requirements

6.9.2.1 The material used inside the metal capof the product shall conform to the relevantIndian Standards of food grade plastics aspermitted under the Prevention of FoodAdulteration Act, 1954 and the Rules madethereunder. Caps and closures shall not betreated as labels.

6.9.2.2 No synthetic food colour and artificialsweetener shall be added or used in theproduct.

6.9.2.3 Product shall be free from Aflatoxinswhen tested in accordance with the methodprescribed in Appendix J of IS 4684 : 1975.

7 PACKING AND MARKING

7.1 Packing

The product shall be packed in hermeticallysealed, clean and sound metal containers( see IS 11078 : 1984 ) or in a flexible pack so asto protect it from deterioration. In case plasticmaterial is used for flexible packaging, onlyfood grade plastic shall be used( see IS 10171 : 1987 ).

7.1.1 The product shall be packed in nitrogen ora mixture of nitrogen and carbon dioxide.

7.2 The product shall be packed in quantities asstipulated under Rule 5 and ‘The ThirdSchedule’ of the Standards of Weights andMeasures ( Packaged Commodities ) Rules, 1977as well as in accordance with requirementsunder PFA Act 1954 and Rules 1955.

7.3 Marking

The containers shall bear legibly and indeliblythe following information:

a) Name of the material, and brand name, ifany;

b) Type of material;

c) Name and address of the manufacturer;d) Batch or code number;e) Month and year of manufacturing or

packing;f) Net mass ( see 7.2 );g) Date before which the contents should be

consumed, be indicated by marking thewords ‘Use before............. (month andyear);

h) Composition — Indicating the approximatecomposition of nutrients per 100 g of theproduct as well as the energy value injoules;

j) Feed chart and directions for use; andk) Any other requirements as stipulated

under

7.3.1 In case of flexible packs, a cautionarynotice to the following effect shall be printed onthe container:

“On opening, transfer the contents of thepack to a clean air tight container. After eachuse, replace the lid tightly and store in a cooldry place”.

7.3.2 BIS Certification Marking

The product may also be marked with theStandard Mark.

7.3.2.1 The use of the Standard Mark isgoverned by the provisions of the Bureau ofIndian Standards Act, 1986 and the Rules andRegulations made thereunder. Details ofconditions under which a license for the use ofthe Standard Mark may be granted tomanufacturers or producers may be obtainedfrom the Bureau of Indian Standards.

7.3.2.2 Eco-Mark

The product may also be marked with theECO-Mark, the details of which may beobtained from Bureau of Indian Standards.

8 SAMPLING

8.1 Representative samples of the materialshall be drawn and tested for conformity to thisstandard as prescribed in Annex E.

i)Rule 37-B of PFA Rules 1955,ii) Infant Milk substitutes, Feeding Bottles

and Infant Foods Act, 1992 and Rules1993; and

iii)Standards of Weights and Measures( Packaged Commodities ) Rules, 1977.

IS 14433 (Part 1) : 1997

4

Table 1 Requirements for Infant Milk Substitutes( Clauses 6.8 and E-4.1 )

SlNo.

Characteristic Requirement Method of Test, Ref to

Type I Type II(1) (2) (3) (4) (5)

i) Moisture, g/100 g, Max 4.5 4.5 IS 11623:1986ii) Milk protein, g/100 g: IS 7219:1973

Min 12.0 10.0Max — 16.0

iii) Fata) Milk fat, g/100 g, Min 18.0 12.0 IS 11721:1986b) Total fat, g/100 g, Min — 18.0 do

iv) Total ash, g/100 g, Max 8.5 6.0 Annex Bv) Acid, insoluble ash, g/100 g,

Max0.1 0.1 Annex C

vi) Insolubility index,ml/100 g, Maxfor roller driedfor spray dried

15.02.0

15.02.0

IS 12759 : 1989

vii) Vitamin A(as retinol),ug/100 g, Min

350 350 IS 5886:1970

viii) Iron, mg/100 g, Min 5.0 5.0 Annex Dix) Heavy metals

a) Lead, mg/kg, Max 0.2 0.2 IS 12074 : 1987b) Arsenic, mg/kg, Max 0.05 0.05 IS 11124 : 1984c) Tin, mg/kg, Max 5.0 5.0 17 of IS 2860 :

1964d) Cadmium, mg/kg, Max 0.1 0.1 15 of IS 1699 :

1995x) Added vitamin D

(expressed as chole-calciferol)IU/100 g, Min

180 180 IS 5835 : 1970

xi) Thiamine µg/100 g, Min 185 185 IS 5398 : 1969xii) Nicotinamide µg/100 g, Min 1 160 1 160 IS 5400 : 1969

xiii) Riboflavin µg/100 g, Min 275 275 IS 5399 : 1969xiv) Vitamin B6 µg/100 g, Min 160 160 IS 7530 : 1975xv) Vitamin B12 µg/100 g, Min 0.7 0.7 IS 7529 : 1975

xvi) Folic acid µg/100 g, Min 20 20 IS 7234 : 1974xvii) Pantothenic acid, mg/100 g, Min 1.4 1.4 IS 9840 : 1981

xviii) Biotin, µg/100 g, Min 7 7 IS 9820 : 1981xix) Vitamin C, mg/100 g, Min 35 35 IS 5838 : 1970xx) Vitamin K, µg/100 g, Min 18 18 *

xxi) Calcium, mg/100 g, Min 230 230 IS 5949 : 1990xxii) Phosphorus, mg/100 g, Min 115 115 IS 12756 : 1989

xxiii) Iodine, µg/100 g, Min 20 20 A-2 of IS 7224 : 1985

xxiv) Copper, µg/100 g, Min 280 280 15 of IS 1699 : 1995

xxv) Manganese, µg/100 g, Min 20 20 35 of IS 3025 : 1964

xxvi) Zinc, mg/100 g, Min 2.5 2.5 15 of IS 1699 : 1995

xxvii) Sodium, mg/100 g, Min 90 90 IS 12760 : 1989xxviii) Potassium, mg/100 g, Min 370 370 do

xxix) Chloride, mg/100 g, Min 250 250 IS 11763 : 1986xxx) Magnesium, mg/100 g, Min 22 22 IS 5949 : 1990

xxxi) Choline, mg/100 g, Min 32 32 *

IS 14433 (Part 1) : 1997

5

ANNEX A( Clause 2 )

LIST OF REFERRED INDIAN STANDARDS

Table 1 ( Concluded )

NOTES

1 For the purpose of Type tests, all tests mentioned above are to be carried out and for the purpose of Routine tests, thetests given from Sl No. (i) to (viii) are to be carried out.

2 The Indian Standards on methods for test indicated in col 5 from Sl No.(x) to (xviii) are given for guidance only as theyare under revision at present. As there is no other suitable and easily workable method at present, the manufacturerswould be required to maintain a record showing the quantity of these ‘added vitamins’, added to each batch.

3 In case of Type II infant milk substitutes, since there is no reliable method at present for the estimation of separatecontents of milk fat (12 percent min) and vegetable fat in the total fat, records of their addition shall be maintained bythe manufacturer. However, the product shall not have less than 18 percent total fat when tested as perIS 11721 : 1986, as mentioned above.* Test method to be specified. Till such time test methods are prescribed, factory records shall be maintained of theadditions per batch.

IS No. Title

1070 : 1992 Reagent grade water( third revision )

1656 : 1997 Milk-cereal based weaningfoods — Specification( third revision )

1699 : 1995 Methods of sampling andtest for food colours( second revision )

2491 : 1972 Code for hygienicconditions for foodprocessing units ( firstrevision )

2860 : 1964 Methods of sampling andtest for processed fruitsand vegetables

3025 : 1964 Method of sampling andtest (physical andchemical) for water used inindustry

4684 : 1975 Specification of ediblegroundnut flour (expellerpressed) ( first revision )

4905 : 1968 Method for randomsampling

5055 : 1996 Lecithin, food grade ( firstrevision )

5398 : 1969 Method for estimation ofthiamine (vitamin B-1) infoodstuffs

5399 : 1969 Methods for estimation ofriboflavin (vitamin B-2) infoodstuffs

5400 : 1969 Methods for estimation ofnicotinic acid (Niacin) in

IS No. Title

foodstuffs5401 : 1969 Method for detection and

estimation of coliformbacteria in foodstuffs

5402 : 1969 Method for plate count ofbacteria in foodstuffs

5403 : 1969 Method for yeast andmould count of foodstuffs

5835 : 1970 Method for estimation ofvitamin D in foodstuffs

5838 : 1970 Method for estimation ofVitamin C in foodstuffs

5886 : 1970 Methods for estimation ofcarotenes and Vitamin A(Retinol) in foodstuffs

5887 Methods for detection ofbacteria responsible forfood poisoning

(Part 1) : 1976 Isolation, identification andenumeration of Escherichiacoli ( first revision )

(Part 2) : 1976 Isolation, identificationand enumeration ofStaphylococcus aureus andfaecal streptococci ( firstrevision )

(Part 3) : 1976 Isolation and identificationof Salmonella and Shigella( first revision )

(Part 5) : 1976 Isolation and identificationof Vibrio Cholerae andVibrio Parahaemolyticus( first revision )

IS 14433 (Part 1) : 1997

6

ANNEX B[Table 1, Sl No. (iv)]

DETERMINATION OF TOTAL ASH

B-1 APPARATUS

B-1.1 Flat-Bottom Dish — of stainless steel,porcelain, silica or platinum.

B-1.2 Muffle Furnace — maintained at 550 ±20°C.

B-1.3 Desiccator

B-2 PROCEDURE

B-2.1 Weigh accurately 3 g of the material inthe dish, previously dried in an air-oven andweighed. Heat the dish gently on a flame atfirst and then strongly in a muffle furnace tillgrey ash results. Cool the dish in a desiccatorand weigh. Heat the dish again for 30 minutesin the muffle furnace. Cool the dish in adesiccator and weigh. Repeat this process ofheating for 30 minutes, cooling and weighinguntil the difference between two successive

IS No. Title5949 : 1990 Method for volumetric

determination of calciumand magnesium usingEDTA ( first revision )

6387 : 1987 Vegetable protein infantfood with milk ( firstrevision )

7219 : 1973 Method for determinationof proteins in food and feedingredients

7224 : 1985 Iodized salt ( first revision )7234 : 1974 Method for estimation of

folic acid in foodstuffs7235 : 1974 Estimation of tocopherols

(vitamin E) in foodstuffs7529 : 1975 Method for estimation of

vitamin B12 in foodstuffs7530 : 1975 Method for estimation of

pyridoxine (vitamin B6) infoodstuffs

9820 : 1981 Method for estimation ofbiotin in foodstuffs

9840 : 1981 Method for estimation ofpantothenic acid infoodstuffs

10171 : 1987 Guide on suitability ofplastics for food packaging( first revision )

10641 : 1983 Recommended methods fordetermination of aromaand taste thresholds

11078 : 1993 Round open top sanitarycans for milk powder ( firstrevision )

11124 : 1984 Method for atomicabsorptionspectrophotometricdetermination of arsenic

IS No. Title

11546 : 1985 Methods of sampling formilk and milk products

11623 : 1986 Method for determinationof moisture content in milkpowder and similarproducts

11721 : 1986 Determination of fatcontent in milk powder andsimilar products (routinemethod)

11763 : 1986 Methods for determinationof chloride content by thepotentiometric titrationmethod in cheese andprocessed cheese products

12074 : 1987 Method for determinationof lead byatomic absorptionspectrophotometry

12756 : 1989 Cheese and cheeseproducts — Determinationof total phosphorus contentby molecular absorptionspectrometric method

12759 : 1989 Dried milk and dried milkproducts — Determinationof insolubility index.

12760 : 1989 Dried Milk —Determination of sodiumand potassium contents —Flame emissionspectrometric method

13462 : 1992 Ascorbyl palmitate, foodgrade

13500 : 1992 Spray dried milk powders— Scorched particles —Determination

IS 14433 (Part 1) : 1997

7

weighings is less than one milligram. Recordthe lowest mass.

NOTE — Preserve the dish containing the ash for thedetermination of acid insoluble ash ( see C-3 ).

B-3 CALCULATIONB-3.1 Total ash, percent by mass

=

where

ANNEX C[Table 1, Sl No. (v)]

DETERMINATION OF ACID INSOLUBLE ASH

C-1 APPARATUS

C-1.1 Flat-Bottom Dish — of stainless steel,porcelain, silica or platinum.C-1.2 Muffle Furnace — maintained at 550 ±20°C.C-1.3 Desiccator

C-2 REAGENT

C-2.1 Dilute Hydrochloric Acid — 5 Nprepared from concentrated hydrochloric acid.

C-3 PROCEDURE

C-3.1 To the ash contained in the dish ( seeNOTE under B-2.1 ), add 25 ml of dilutehydrochloric acid. Cover with a watch-glass andheat on a water bath for 10 minutes. Allow tocool and filter the contents of the dish througha Whatman filter paper No. 42 or itsequivalent. Wash the filter paper with wateruntil the washings are free from the acid andreturn it to the dish. Keep it in an oven

maintained at 100 ± 2°C for about 3 hours.Ignite in a muffle furnace at 550 ± 20°C for onehour. Cool the dish in a desiccator and weigh.Heat the dish again at 550 ± 20°C for 30minutes, cool in a desiccator and weigh. Repeatthis process for heating for 30 minutes, coolingand weighing until the difference between twosuccessive weighings is less than onemilligram. Record the lowest mass.

C-4 CALCULATION

C-4.1 Acid insoluble ash,

percent by mass =

ANNEX D[Table 1, Sl No. (viii)]

DETERMINATION OF IRON

D-0 GENERAL

The determination of iron may be carried outeither by the spectrophotometric method at D-1or by Wong’s spectrocolorimetric method at D-2.In case of a dispute, the Spectrophotometricmethod at D-1 shall be used.

D-1 SPECTROPHOTOMETRIC METHOD

D-1.1 Glassware, including pipettes, should becleaned with re-distilled nitric acid andthoroughly rinsed with re-distilled water.Portions of glassware which come in contactwith the material should not be permitted tocome in contact with any surface that maycause contamination, for example, table tops,racks, iron stand, operators’ hands, etc.

100 M2 M –( )M1 M–

-----------------------------------------

M2 = mass in g, of the dish with the ash;

M = mass, in g, of the empty dish; and

M1 = mass, in g, of the dish with thematerial taken for the test.

where

M2 = mass in g, of the dish with the acidinsoluble ash;

M = mass, in g, of the empty dish, andM1 = mass, in g, of the dish with the

material taken for the test.

100 M2 M –( )M1 M–

-----------------------------------------

IS 14433 (Part 1) : 1997

8

D-1.2 All the reagents should be stored inneutral ground glass-stoppered bottles.

D-1.3 Apparatus

D-1.3.1 Volumetric Flasks — 100-ml and 25-ml.

D-1.3.2 One-Mark Graduated Flask — 100-mlcapacity.

D-1.3.3 Separating Funnel — 125-ml capacity.

D-1.3.4 Graduated Glass Measuring Cylinder( Stoppered ) — 25-ml capacity.

D-1.3.5 A Suitable Spectrophotometer orPhotoelectric Colorimeter — adjusted fortransmission at 485 nm.

D-1.4 Reagents

D-1.4.1 Hydrochloric Acid — 20 percent( m/m ).

D-1.4.2 Re-distilled Nitric Acid — sp gr 1.42.

D-1.4.3 Concentrated Hydrochloric Acid — spgr 1.16.

D-1.4.4 Distilled Water ( see IS 1070 : 1992 ).

D-1.4.5 Bromine Water — a saturated solutionof bromine in water.

D-1.4.6 Dilute Hydrochloric Acid — 1 : 1( m/m ).

D-1.4.7 Potassium Persulphate Solution — 2percent ( m/m ) in distilled water ( see IS 1070 :1992 ), prepared freshly every few days andstored under refrigeration.

D-1.4.8 Potassium Thiocyanate Solution — 20percent ( m/m ) in distilled water ( see IS 1070 :1992 ), prepared freshly every few days andstored under refrigeration.

D-1.4.9 Isobutyl Alcohol — boiling point 106 to107°C, redistilled in neutral glass apparatus(reagent recovered by simple distillation is notsatisfactory for reuse).

D-1.4.10 Anhydrous Sodium Sulphate

D-1.5 Preparation of the Standard Curve

D-1.5.1 Weigh accurately 1.000 g of iron wireinto a clean, dry, iron-free beaker. Dissolve it inhydrochloric acid, sufficient to dissolve it, towhich 1 to 2 millilitres of nitric acid have beenadded. Carefully evaporate to dryness anddissolve the residue in the minimum amount ofconcentrated hydrochloric acid. Transfer it to a100-ml volumetric flask and dilute to volume.

D-1.5.2 From the above stock solution, preparea working standard of 10 micrograms iron permillilitre by diluting with distilled water ( seeIS 1070 : 1992 ). Add a few drops of bromine

water prior to adjusting to volume. Draw astandard curve by developing the colour onincrements of the working standard in therange of 0 to 60 micrograms of iron by taking ina 25-ml volumetric flask, 5 ml of concentratedhydrochloric acid, the required quantity ofstandard iron solution and making up to thevolume by distilled water ( see IS 1070 : 1992 ).Proceed as in D-1.6.2.

D-1.6 Procedure

D-1.6.1 Weigh accurately 3 to 5 g of thematerial in a silica, porcelain or platinum dish.Char the sample at low heat. Place the charredsample in a muffle furnace at 550 ± 20°C for aperiod of about 5 hours for ashing. Aftercooling, dissolve the ash by adding 5 ml ofdilute hydrochloric acid and heating themixture to a gentle boil for 3 minutes. Allow thecontents to cool to room temperature. Transferthe contents to a 100-ml one-mark graduatedflask and dilute to volume with distilled water( see IS 1070 : 1992 ).D-1.6.2 Transfer 25-ml aliquot of the preparedsolution to a 125-ml separating funnel and addexactly 5 ml of concentrated hydrochloric acid.Add one ml of potassium persulphate solutionand swirl the separating funnel to ensurecomplete mixing. Then add 10 ml of potassiumthiocyanate solution to develop the colour. Add25 ml of isobutyl alcohol and shake for twominutes. Draw off and discard the aqueouslayer. Invert and then slowly revolve the funnelto dislodge any water particles sticking to thewalls of the separating funnel. Allow to standfor 10 minutes. After this period draw off thesmall amount of water which has separatedfrom the alcohol layer and then transfer thisalcohol layer to a dry 25-ml graduatedmeasuring cylinder. Add about 0.1 g anhydroussodium sulphate to the contents of this cylinderand agitate it to ensure the removal ofsuspended particles of water from the alcoholextract.D-1.6.3 Determine the transmittance of thealcohol extract in a spectrophotometer orphoto-electric calorimeter at 485 nm set with areagent blank at 100 percent transmittance.The reagent blank is prepared in the samemanner as the sample.

NOTE — If the colour is too intense to read (in excess of50 micrograms) repeat the determination, using asmaller aliquot of the prepared sample. It is importantthat the volume ratio and prepared sample — blankrelationship be kept constant. The difference in thealiquot size should be made up by the addition of thereagent blank solution. For example, if a 15-ml aliquotis used in place of the usual 25 ml, correct the differencein volume by adding 10 ml of the reagent blank.

D-1.7 Calculation

IS 14433 (Part 1) : 1997

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D-1.7.1 Find out the amount of iron present, interms of micrograms in the solution, by plottingthe intensity reading on the standard curvepreviously drawn ( see D-1.5.2 ) and calculatethe quantity of iron as mg per 100 g of sample.

D-2 WONG’S SPECTROCOLORIMETRIC METHOD

D-2.1 Principle

D-2.1.1 Iron is determined colorimetricallymaking use of the fact that ferric iron gives ablood red colour complex with potassiumthiocyanate whose intensity is measured at500 nm.D-2.2 Reagents

D-2.2.1 Sulphuric Acid — 30 percent ( m/v ).D-2.2.2 Potassium Persulphate Solution — 7percent ( m/v ). Dissolve 7 g potassiumpersulphate in distilled water ( see IS 1070 :1992 ), and make volume upto 100 ml.D-2.2.3 Potassium Thiocyanate Solution — 40percent ( m/v ). Dissolve 40 g potassiumthiocyanate in distilled water ( see IS 1070 :1992 ). Add 4 ml acetone and make up thevolume to 100 ml.D-2.2.4 Standard Iron Solution — Dissolvepure iron or ammonium ferrous sulphate andmake appropriate dilution so as to get asolution of iron concentration of 20 µg/ml.

D-2.3 Procedure

D-2.3.1 Preparation of Sample Solution — SeeD-1.6.1.D-2.3.2 Estimation of IronD-2.3.2.1 Transfer suitable volume (2 to 4 ml)of the prepared sample solution (D-2.3.1) intothe measuring cell using pipette. Add therequired quantity of distilled water ( seeIS 1070 : 1992 ) so that the total volume is6.5 ml. Add 1 ml sulphuric acid, 1 ml potassiumpersulphate solution and 1.5 ml of potassiumthiocyanate solution. Shake well and measurethe optical density (O.D) of the developed colourwithin 20 minutes, colorimetrically, at 500 nmusing a suitable Spectrocolorimeter. Similarly,find out the standard optical density (O.D)using standard iron solution (D-2.2.4) in placeof prepared sample solution.D-2.4 Calculation

D-2.4.1 Calculate the quantity of iron asmilligram per 100 g of sample using thefollowing formulae:

Iron, mg/ 100 g

= ×

ANNEX E( Clause 8.1 )

SAMPLING OF INFANT MILK SUBSTITUTES

E-1 GENERAL REQUIREMENTS

E-1.0 In drawing, preparing, storing andhandling samples, the following precautionsand directions shall be observed.

E-1.1 Samples shall be taken in a protectedplace not exposed to damp air, dust or soot.

E-1.2 The sampling instrument shall be cleanand dry when used. When taking samples formicrobiological examination, it shall be sterile.

E-1.3 Precautions shall be taken to protect thesamples, the material being sampled, thesampling instrument and the containers for

samples from adventitious contamination.

E-1.4 The samples shall be placed in clean anddry glass containers. The sample containersshall be of such a size that they are almostcompletely filled by the sample. The samplecontainers shall in addition be sterile whenthey are used for samples for microbiologicalexamination.

E-1.5 Each container shall be sealed air-tightafter filling and marked with full details ofsampling, batch or code number, name of themanufacturer and other important particularsof the consignment.

Standard Conc.Standard O. D.------------------------------------------- Sample O. D.

Aliquot taken--------------------------------------×

Volume madeSample taken-------------------------------------- 100

1 000---------------×

IS 14433 (Part 1) : 1997

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E-1.6 Samples shall be stored in such a mannerthat the temperature of the material does notvary unduly from the normal temperature.

E-2 SCALE OF SAMPLING

E-2.1 Lot

E-2.1.1 All the containers in a singleconsignment of one type of material drawnfrom a single batch of manufacture shallconstitute a lot. If the consignment is declaredto consist of different batches of manufacture,the batches shall be marked separately and thegroup of containers in each batch shallconstitute separate lots.

E-2.1.2 Samples shall be tested for each lotascertaining its conformity to the requirementsof this standard.

E-2.2 The number of containers to be selectedfrom the lot shall depend on the size of the lotand shall be as given in Table 2.

E-2.3 The containers shall be chosen at randomfrom the lot. In order the ensure therandomness of selection, procedures as given inIS 4905 : 1968 may be followed.

E-3 TEST SAMPLES AND REFEREE SAMPLES

E-3.1 The number of containers selectedaccording to col 2 of Table 2 shall be randomlydivided into two groups, Group A and Group Bunder col 3 and 4. The number of containers inGroup A shall be used for testingcharacteristics other than microbiological andthe containers in Group B shall be used fortesting microbiological specifications.

E-3.2 Draw with the suitable samplinginstrument approximately equal quantity of

material from different parts of each containerin Group A till about 300 g of material isobtained. The quantity of material so obtainedshall be thoroughly mixed and divided intothree equal parts. Each part so obtained shallconstitute an individual sample representingthe container and shall be transferredimmediately to thoroughly clean and drysample container, sealed air-tight and labelledwith the particulars given in E-1.5. Theindividual sample so obtained shall be dividedinto three sets in such a way that each set has asample representing each selected container.One of these sets shall be marked for thepurchaser, another for the vendor and the thirdfor the referee.

E-3.3 From the material from each selectedcontainer, remaining after the individualsample has been taken, approximately equalquantities of material shall be taken and mixedthoroughly so as to form a composite sampleweighing about 300 g. This composite sampleshall be divided into three equal parts andtransferred to clean add dry containers sealedair-tight and labelled with the particulars asgiven in E-1.5. One of these composite samplesshall be for the purchaser, another for thevendor and the third for the referee.

E-3.4 From each of the container in Group B,draw with a suitable sampling instrumentwhich is sterile; at least 150 g of material andmix thoroughly in aseptic conditions to form asample for microbiological examination. Dividesample (taking care not to bring anymicrobiological contamination in the material)into three equal parts. Each part so obtainedshall constitute a sample representing thecontainer and shall be transferred to sterileglass containers and shall be sealed air-tightand labelled with the particulars givenin E-1.5. They shall be marked, in addition,with the words, ‘For microbiologicalExamination’. The sample so obtained shall bedivided into three sets in such a way that eachset has a sample representing each selectedcontainer. One of these sets shall be marked forthe purchaser, another for the vendor and thethird for the referee.

E-3.5 Referee Sample

Referee sample shall consist of a set ofindividual samples (E-3.1), a composite sample(E-3.2) and a set of samples for microbiologicalexamination (E-3.3) marked for this purposeand shall bear the seals of the purchaser andthe vendor. These shall be kept at a place asagreed to between the two so as to be used incase of a dispute.

Table 2 Scale of Sampling for Containers of 400 g and Above

Number of Containers in the Lot

Number of Containersto be Selected

Total Group A Group B(1) (2) (3) (4)

50 to 100 3 2 1101 to 300 5 3 2301 to 500 7 4 3501 and above 9 5 4

NOTES

1 The scale of sampling for containers of 200 g shall beas agreed to between the purchaser and the supplier.

2 The scale of sampling for less than 50 containers of400 g in a lot shall be as agreed to between thepurchaser and the supplier.

IS 14433 (Part 1) : 1997

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E-4 NUMBER OF TESTS

E-4.1 Tests for determination of moisture, totalmilk protein, milk fat, total fat, total ash, acidinsoluble ash and insolubility index as given inTable 1 shall be conducted on each of thesamples constituting a set of individualsamples.

E-4.2 Tests for microbiological specificationsshall be conducted on each of the samplesconstituting a set of test samples labelled withthe words ‘For Microbiological Examination’.E-4.3 Tests other than those given in E-4.1and E-4.2 shall be conducted on the compositesample.

Bureau of Indian Standards

BIS is a statutory institution established under the Bureau of Indian Standards Act, 1986 to promoteharmonious development of the activities of standardization, marking and quality certification of goods andattending to connected matters in the country.

Copyright

BIS has the copyright of all its publications. No part of these publications may be reproduced in any formwithout the prior permission in writing of BIS. This does not preclude the free use, in the course ofimplementing the standard, of necessary details, such as symbols and sizes, type or grade designations.Enquiries relating to copyright be addressed to the Director (Publications), BIS.

Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are alsoreviewed periodically; a standard along with amendments is reaffirmed when such review indicates that nochanges are needed; if the review indicates that changes are needed, it is taken up for revision. Users ofIndian Standards should ascertain that they are in possession of the latest amendments or edition byreferring to the latest issue of ‘BIS Catalogue’ and ‘Standards : Monthly Additions’.

This Indian Standard has been developed from Doc : No. FAD 57 (516)

Amendments Issued Since Publication

Amend No. Date of Issue

Amd. No. 1 November 1997

Amd. No. 2 December 1998

BUREAU OF INDIAN STANDARDS

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